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Method for preparing antidepressant fluoxetine

A technology for medicine fluoxetine and antidepressant, applied in the field of preparation of pharmaceutical compounds, can solve problems such as environmental pollution of fluoxetine, achieve the effects of improving reaction conversion rate, facilitating reaction speed and reducing environmental pollution

Inactive Publication Date: 2011-02-02
WENZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0023] The invention provides a method for preparing the antidepressant fluoxetine to solve the environmental pollution caused by multi-step separation in the current production process of fluoxetine

Method used

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  • Method for preparing antidepressant fluoxetine
  • Method for preparing antidepressant fluoxetine
  • Method for preparing antidepressant fluoxetine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1.68g (0.01mol) of β-chloropropiophenone was put into the high-pressure reactor lined with polytetrafluoroethylene, and 10ml of deoxidized i-C 3 h 7 OH solvent, seal the reactor, replace the air in the reactor with nitrogen for 3 times, replace the nitrogen with methylamine gas for 3 times, adjust the pressure of the reactor to 0.1MPa, turn on the stirrer, slowly raise the temperature to 80°C, and after 12 hours of reaction, drop to to room temperature, replace the gas in the reaction system with nitrogen for 3 times, open the reaction kettle, and put Ru / γ-Al 2 o 3 Support the catalyst (the preparation of the catalyst has been described in the 200910095808.1 patent specification), add 0.056g (0.001mol) of KOH, and seal the autoclave.

[0045] Use high-purity nitrogen to replace the air in the high-pressure reactor for 3 times, and then use hydrogen to replace the nitrogen for 3 times, then fill the hydrogen to 1MPa, the reaction temperature is 100°C, and react for 10 ...

Embodiment 2

[0049] 2.52g (0.015mol) β-chloropropiophenone is put into the high-pressure reactor of lining polytetrafluoroethylene, adds the tetrahydrofuran solvent of 20ml, seals the reactor, replaces the air in the reactor with nitrogen for 5 times, passes through methanol Replace the nitrogen with amine for 5 times, adjust the pressure of the reactor to 0.5MPa, turn on the stirrer, slowly raise the temperature to 100°C, react for 10 hours, then cool down to room temperature, replace the gas in the reaction system with nitrogen for 5 times, and put Ru-Pd / γ-Al 2 o3 Support the catalyst (the preparation of the catalyst has been described in the 200910095808.1 patent), add 0.040 g (0.001 mol) of NaOH, and seal the autoclave.

[0050] Use high-purity nitrogen to replace the air in the high-pressure reactor for 5 times, and then use hydrogen to replace the nitrogen for 5 times, then fill the hydrogen to 1.2MPa, the reaction temperature is 120°C, and react for 6 hours. During the reaction, the ...

Embodiment 3

[0053] 3.36g (0.02mol) β-chloropropiophenone is put into the high-pressure reactor lined with polytetrafluoroethylene, add 20ml of dimethylformamide solvent, seal the reactor, and replace the air in the reactor with nitrogen for 5 times , feed methylamine to replace nitrogen 5 times, adjust the pressure of the reactor to 0.4MPa, turn on the stirrer, slowly raise the temperature to 60°C, after 11 hours of reaction, lower the reaction temperature to room temperature, replace the gas in the reaction system with nitrogen 5 times, put in Rh / γ-Al 2 o 3 Loaded catalyst (the preparation of the catalyst has been described in the 200910095808.1 patent), add 0.106g (0.001mol) of Na 2 CO 3 , Sealed autoclave.

[0054] Use high-purity nitrogen to replace the air in the high-pressure reactor for 5 times, and then use hydrogen to replace the nitrogen for 5 times, then fill the hydrogen to 1.5MPa, the reaction temperature is 60°C, and react for 8 hours. During the reaction, the hydrogen p...

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Abstract

The invention relates to a method for preparing antidepressant fluoxetine, and belongs to the method for preparing a medicinal compound. The technical scheme in the invention comprises the following three steps of aminolysis, catalytic hydrogenation and aromatic etherification reaction, wherein the three steps are performed in one pot without separation. In the method, the conventional chemical reduction method is replaced by the catalytic dehydration process, and the used reducing agent is hydrogen gas, so that the environmental pollution is reduced; the methylamine is gaseous methylamine, so that the reaction conversion rate is improved, and other substances, such as water and the like, are prevented from being introduced into a reaction system; and p-chlorobenzotrifluoride is added dropwise in the etherification reaction, so that the reaction speed can be conveniently controlled, the yield of a target product is improved, and the possibility of catalyst poisoning is reduced.

Description

technical field [0001] The invention belongs to a preparation method of a pharmaceutical compound, in particular to a method for preparing the antidepressant fluoxetine. Background technique [0002] Among the commonly used antidepressants, fluoxetine plays an important role. These drugs have definite curative effect, few side effects, good tolerance and good patient compliance, and are deeply accepted by clinicians and patients. The chemical name of fluoxetine is N-methyl-γ-[4-(trifluoromethyl)-phenoxy]-amphetamine hydrochloride, and its structure is as the structural formula. [0003] [0004] The initial process for preparing fluoxetine is to use 3-dimethylamino-1-phenylpropanol as raw material, chlorinated by thionyl chloride, and etherified with p-trifluoromethylphenol to obtain N-methyl fluoride Xitine, then carry out demethylation with ethyl chloroformate, hydrolysis, salt-forming reaction to generate fluoxetine hydrochloride, its process is as follows: [0005]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/48C07C213/06
Inventor 赵亚娟李丹丹何道法黄幸王玉祥任宝东
Owner WENZHOU UNIVERSITY
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